反应详情

To a solution of 95 mg of 1-(t-butoxycarbonyl)-4-(6-bromo-imidazo[1,2-a]pyridin-3-yl)-piperidine (from Example 274, Step A), and 158 mg of tributyl(vinyl)tin in 6 mL toluene was added 5.3 mg of dichlorobis (triphenyl phosphine)-palladium(II). The mixture was refluxed for 2 hours. The reaction was cooled down to r.t. and partitioned between CH2Cl2and water. Aqueous layer was extracted with CH2Cl2 (3×). The combined organic phase was washed with brine and dried over MgSO4. After concentration, the residue was purified by prep TLC (100% EtOAc) to give 90 mg of the title compound as a viscous oil, which was used in next step without further purification.

1. temperatureThe mixture was refluxed for 2 hours
2. custompartitioned between CH2Cl2and water
3. extractionAqueous layer was extracted with CH2Cl2 (3×)
4. washThe combined organic phase was washed with brine
5. dry with materialdried over MgSO4
6. concentrationAfter concentration
7. customthe residue was purified by prep TLC (100% EtOAc)